Sensitive and selective spectrophotometric determination of palladium(II) ion following its preconcentration using modified magnetite nanoparticles and 3-phasic backextraction

We report on a method for selective extraction and backextraction for the ultra-sensitive determination of Pd(II). Magnetite nanoparticles modified with sodium dodecyl sulfate were used to extract Pd(II) as its green 1-(2-pyridylazo)-2-naphtholate complex prior to zero- and first-derivative spectrophotometric determination at 659 and 681?nm, respectively. A sample volume of 70?mL was backextracted with 0.50?mL of n-butanol in a 3-phasic system. The effects of reaction time and the other variables were optimized. The enrichment factor is 134 and the calibration plots are linear in the range from 2 to 90?ng?mL^-1 of Pd(II). The detection limit is 0.3?ng?mL^-1 and the relative standard deviations and recoveries at levels of 10 and 72?ng?mL^-1 of Pd(II) are in the range from 1.1?C4.9%, and from 98.5?C102.6%, respectively. Most ions do not significantly interfere. The method was successfully applied to the determination of Pd(II) in water and urine samples, alloys, and palladium catalysts.

Probing the intestinal α-glucosidase enzyme specificities of starch-digesting maltase-glucoamylase and sucrase-isomaltase: synthesis and inhibitory properties of 3'- and 5'-maltose-extended de-O-sulfonated ponkoranol

The synthesis and glucosidase inhibitory activities of two C-3'- and C-5'-β-maltose-extended analogues of the naturally occurring sulfonium-ion inhibitor, de-O-sulfonated ponkoranol, are described. The compounds are designed to test the specificity towards four intestinal glycoside hydrolase family 31 (GH31) enzyme activities, responsible for the hydrolysis of terminal starch products and sugars into glucose, in humans. The target sulfonium-ion compounds were synthesized by means of nucleophilic attack of benzyl protected 1,4-anhydro-4-thio-D-arabinitol at the C-6 position of 6-O-trifluoromethanesulfonyl trisaccharides as alkylating agents. The alkylating agents were synthesized from D-glucose by glycosylation at C-4 or C-2 with maltosyl trichloroacetimidate. Deprotection of the coupled products by using a two-step sequence, followed by reduction afforded the final compounds. Evaluation of the target compounds for inhibition of the four glucosidase activities indicated that selective inhibition of one enzyme over the others is possible.     

Zinc and copper oxide nanoparticles decrease synaptosomal glutamate uptake: an in vitro study

Nanoparticles (NPs) are considered as an important environmental risk factor for cognitive impairments and neurodegenerative disorders. Recent evidences have reported a glutamatergic system response against air-borne NPs. Zinc and copper oxides (ZnO and CuO) NPs are the most common metal oxide NPs in industries. The effects of these NPs on hippocampal voltage-dependent ion channels and spatial cognition have been previously studied. However, there is a lack of evidence regarding the effects of ZnO and CuO NPs on glutamatergic synapse neurotransmission in central nervous system. In the present study, the effects of ZnO and CuO NPs on glutamate (Glu) release and uptake have been investigated in isolated nerve terminals (synaptosomes). Our findings have shown that, even in high doses of ZnO and CuO NPs, no significant effect on Glu release is observed. However, a decrease has been observed in uptake of Glu. Hence, ZnO and CuO NPs can be considered as hazardous agents inducing neurodegenerative disorders through Glu excitotoxicity.     

Simultaneous determination of cobalt and palladium in micellar media using H-point standard addition method and partial least square regression

A simple, sensitive and selective spectrophotometric method for the simultaneous determination of Co(II) and Pd(II) using partial least square (PLS) calibration and H-point standard addition method is described. The method is based on the complex formation of Co(II) and Pd(II) with 4-(2-pyridylazo) resorcinol (PAR) in acidic media and in the presence of sodium dodecyl sulfate (SDS) as a micellizing agent. Acidic media and the presence of a micellar system improve selectivity and sensitivity, respectively. By applying PLS calibration, Co(II) and Pd(II) can be determined in the range of 0.20-2.0 and 0.40-4.0 microg ml(-1), respectively. The relative errors of prediction for the determination of Co(II) and Pd(II) in the 10 prediction samples were 1.69 and 1.72%, respectively. The results of applying H-point standard addition method show that Co(II) and Pd(II) can be determined simultaneously with concentration ratio of Co(II) to Pd(II) varying between 7:1 and 1:8 in the mixed samples. Both proposed methods (PLS and HPSAM) were applied to the determination of Co(II) and Pd(II) in several alloy solutions with satisfactory results.     

Zero-crossing second derivative spectrophotometry for simultaneous determination of palladium and nickel using 1-(2-pyridylazo)-2-naphthol in mixed micellar solutions

1-(2-Pyridylazo)-2-naphthol (PAN) has been used for the simultaneous determination of nickel and palladium at trace levels. PAN complexes of nickel and palladium in the pH 1.98 form red and green colored complexes, respectively, which are soluble in aqueous 4:1 Triton X-100 to sodium dodecylsulfate (SDS) micellar media with total detergent concentration of 3.2%. Under optimum conditions, calibration graphs for the simultaneous determination by second derivative spectrophotometry were obtained. Zero crossing second derivative spectrophotometry at 668 and 572 nm, respectively for palladium and nickel was used for the simultaneous determination. The method is able to determine palladium to nickel ratio 70:1 to 1:6 (Wt/Wt), accurately. Accuracy and reproducibility of the determination method on the known various amounts of palladium and nickel in their binary mixtures were tested. Effects of diverse ions on the determination of palladium and nickel to investigate selectivity of the method also were studied.     

Extensions of the Lax–Milgram theorem to Hilbert $$C^*$$ C ∗ -modules

Positivity - We present three versions of the Lax–Milgram theorem in the framework of Hilbert $$C^*$$ -modules, two for self-dual ones over $$W^*$$ -algebras and one for those over $$C^*$$...